<p><strong>In the research article recently published in ACS </strong><i><strong>Analytical Chemistry</strong></i><strong> journal the researchers led by Lucie Nováková from the Department of Analytical Chemistry, Faculty of Pharmacy in Hradec Králové, Charles University, present a novel analytical approach for mixtures of natural products.</strong></p><p>This study addresses the complexity of plant extract analysis by developing a holistic two-injection method that integrates <strong>ultrahigh-performance </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?instrumentationItems=38"><strong>supercritical fluid chromatography</strong></a> (<strong>UHPSFC</strong>) with <strong>multimodal ionization tandem mass spectrometry</strong> (<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?instrumentationItems=32"><strong>MS/MS</strong></a>). This method, which does not require manual intervention, significantly improves the efficiency and accuracy of analyzing various small molecules, such as terpenes, flavonoids, and phenolic acids, in plant extracts. The authors applied this method to Eucalyptus sp. extracts, demonstrating its potential as a robust tool for comprehensive plant metabolite analysis.</p><blockquote><h4><strong>The original article</strong></h4></blockquote><blockquote><h5><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.3c03599"><strong>Ultrahigh-Performance Supercritical Fluid Chromatography–Multimodal Ionization–Tandem Mass Spectrometry as a Universal Tool for the Analysis of Small Molecules in Complex Plant Extracts</strong></a></h5><p>Kateřina Plachká, Veronika Pilařová, Štefan Kosturko, Jan Škop, Frantisek Svec, and Lucie Nováková</p><p><i>Analytical Chemistry</i> <strong>2024</strong> <i>96</i> (7), 2840-2848</p><p>DOI: 10.1021/acs.analchem.3c03599</p><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/"><strong>CC-BY 4.0</strong></a></h6></blockquote><h5>Selected sections from the article follow.</h5><h3><strong>Abstract</strong></h3><p>Complex analysis of plant extracts usually requires a combination of several analytical approaches. Therefore, in this study, we developed a holistic two-injection approach for plant extract analysis, which is carried out within one instrument without the need for any manual intervention during the analysis. <strong>Ultrahigh-performance supercritical fluid chromatography</strong> (<strong>UHPSFC</strong>) was employed for the analysis of 17 volatile terpenes on a <strong>porous graphitic carbon column</strong> within 7.5 min, followed by analysis on <strong>short diol column</strong> where flavonoids, phenolic acids, and terpenoic acids were analyzed within 15.5 min. A <strong>multimodal ionization</strong> source <strong>combining </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=electrospray"><strong>electrospray</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=atmospheric+pressure+chemical+ionization"><strong>atmospheric pressure chemical ionization</strong></a> (<strong>ESCi</strong>) was selected for mass spectrometry detection as a simultaneous ionization of both lipophilic and polar compounds was required. The quantitative aspects of the final <strong>UHPSFC-ESI/ESCi-MS/MS two-injection approach</strong> were determined, and it was applied to the <strong>analysis of Eucalyptus sp. extracts</strong> prepared by <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=SFE"><strong>supercritical fluid extraction</strong></a>. Current methods reported in the literature typically require a labor-intensive combination of liquid and gas chromatography for the complex analysis of plant extracts. We present for the first time a new UHPSFC approach requiring only a single instrument that provides an alternative approach to the analysis of complex plant extracts.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Analytical_Chemistry_Analytical_Chemistry_2024_96_7_2840_2848_cover_image_2a6c4c6d6b.jpg" alt="Analytical Chemistry 2024 96 (7), 2840-2848: graphical abstract."></p><h4><strong>Subjects</strong></h4><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=chromatography"><strong>Chromatography</strong></a></li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=Flavonoids"><strong>Flavonoids</strong></a></li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=Hydrocarbons"><strong>Hydrocarbons</strong></a></li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=Ionization"><strong>Ionization</strong></a></li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=Solvents"><strong>Solvents</strong></a></li></ul><h3><strong>Experimental Section</strong></h3><h4><strong>Chromatographic Conditions</strong></h4><p>All experiments were carried out using the supercritical fluid chromatography system <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?instrumentationItems=38&amp;mainauthorItems=5&amp;search=Acquity+UPC2"><strong>Acquity UPC2</strong></a> (Waters, Milford, MA, USA) equipped with a binary pump, an autosampler, a column thermostat, a back pressure regulator (BPR), and a PDA detector. The system was coupled to a triple quadrupole mass spectrometer <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?instrumentationItems=38&amp;mainauthorItems=5&amp;search=Xevo+TQ-XS"><strong>Xevo TQ-XS</strong></a> (Waters) via a commercially available SFC-MS dedicated pre-BPR splitter device with an additional isocratic or binary pump for makeup solvent delivery (Waters).</p><p>Several stationary phases were tested during optimization including Viridis BEH (hybrid silica), Viridis BEH 2-ethylpyridine (2-EP), Torus 2-picolylamine (2-PIC), Viridis HSS C18 SB (C18), Torus 1-amino anthracene (1-AA), all in 3.0 × 100 mm, 1.7 μm, Torus Diol (diol) (3.0 × 50 mm and 100 mm, 1.7 μm), BEH HILIC (2.1 × 100 mm, 1.7 μm), CORTECS HILIC (silica) (3.0 × 100 mm, 1.6 μm), all from Waters, YMC Carotenoid C30 (4.6 × 100 mm, 5 μm) from YMC (Dinslaken, Germany, and porous graphitic carbon (PGC) columns Hypercarb (3.0 × 50 mm and 100 mm, 3.0 μm, Thermo Fisher Scientific Inc., Waltham, MA, USA) and Supel Carbon LC (3.0 × 150 mm, 2.7 μm, Merck KGaA, Darmstadt, Germany). Analyses were carried out using methanolic organic modifiers with or without an additive that included 10 mmol/L ammonia, 5% water, and 10 mmol/L formic acid. Final chromatographic conditions were as follows: Method 1: 150 mm Supel Carbon LC column at 60 °C, BPR pressure at 3300 psi (22.75 MPa), flow rate 1.5 mL/min, MeOH as organic modifier in gradient elution: 0% for 1.5 min, 0–40% in 1.5–4.0 min, 40–41% in 4.0–6.0 min, followed by 1.5 min equilibration at starting conditions. Method 2: 50 mm Torus Diol column at 20 °C and 5% water in MeOH as organic modifier with specific gradient conditions listed in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.3c03599#tbl1"><strong>Table 1</strong></a>. The partial loop with needle overfill injection mode was used to inject 2 and 10 μL samples for methods 1 and 2, respectively. The autosampler was cooled to 5 °C to reduce the evaporation of volatile compounds.</p><h4><strong>MS Conditions</strong></h4><p>The four ionization sources, ESI, APCI, multimodal ESCi, and US, all from Waters were tested. MassLynx Software 4.1 was used for MS control, data acquisition, and processing. Optimization of the ionization sources conditions was carried out using a design of experiment (DoE) approach, followed by the optimization of the makeup solvent composition and flow rate. The makeup solvents tested included pure MeOH and MeOH with various additives, such as water, ammonia, formic acid, and their combinations in different concentrations. The makeup solvent flow rate was tested in the range of 0.0–0.6 mL/min. Selected reaction monitoring (SRM) transitions were determined for each analyte (Supporting Information S2), and their selectivity was verified. MODDE Software 13.0.1 was used to design the experiments for the ion source optimization and subsequent data evaluation. The parameters tested and their respective ranges for each ionization source are listed in Table 2. The DoE were selected as a compromise between the number of experiments required and the power of the study. Three replicates were always included to test the repeatability of the model. The data evaluation included its logarithmic transformation when necessary and the exclusion of outliers to achieve the highest possible linearity (R2), model validity, predictability (Q2), and reproducibility. The limits for the applicable model were set according to the MODDE software: R2 showing model fit &gt;0.5, Q2 estimating future prediction precision &gt;0.1 for significant model and &gt;0.5 for a good model, reproducibility &gt;0.5. Model validity tests diverse model problems and should be &gt;0.25. However, model validity can be lost for very good models with Q2 &gt; 0.9 due to high sensitivity in the test or extremely good replicates (&gt;0.9). Therefore, model validity was always carefully checked manually. The critical factors (marked with “!“ in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.3c03599#tbl2"><strong>Table 2</strong></a>) were identified as having a significant effect on the model, i.e., contributing more than 50% to the final response. Therefore, these factors were optimized separately, and a second DoE was run.</p><h3><strong>Results and Discussion</strong></h3><p>The aim of this study was to develop a holistic method for the simultaneous analysis of compounds typically found in plant extracts, namely, flavonoids, terpenoic and phenolic acids, and terpenes. These compounds include molecules with a wide range of physicochemical properties, from small lipophilic terpenes to polar flavonoids, as listed in Table S1.</p><p>First, a stationary phase had to be selected that would allow the retention of all of the target compounds. We expected that the retention and elution of hydrophilic flavonoids, and especially their glycosylated forms, i.e., rutin, hirsutrin, and hesperidin, would be the main challenge of the UHPSFC-MS method due to the low polarity of the CO₂-based mobile phase. On the other hand, less polar terpenes should be easily retained and eluted. A systematic column screening was carried out on a set of selected stationary phases, including hybrid silica, 2-EP, C18, 2-PIC, and diol with preferred H-bonding and π–π interactions. A generic gradient from 0 to 45% of organic modifier, i.e., MeOH, 10 mmol/L ammonia in MeOH, 10 mmol/L formic acid in MeOH, and 2% water in MeOH, was tested on all five columns. As expected, the addition of water to the organic modifier had a beneficial effect on the elution of polar flavonoids. However, it was necessary to increase the percentage of organic modifiers up to 58% to enable the elution of all target analytes. Unfortunately, these stationary phases were not able to retain most of the lipophilic terpenes, especially those without hydroxy groups. That was surprising as more lipophilic compounds are commonly analyzed by SFC. However, cymene, limonene, pinene, caryophyllene, and citronellal eluted in the dead volume even when using pure CO₂. Volatiles containing hydroxy groups were retained on C18, diol, silica, and 2-EP stationary phases but still coeluted in 1 peak near to the dead volume. Therefore, the retention and separation of terpenes became the main challenge. Accordingly, the 1-AA column with dominant π–π interactions was tested, where the higher retention of nonpolar compounds was expected. This hypothesis was confirmed. However, flavonoids were retained to such an extent that they could not be eluted within a reasonable analysis time under any conditions tested.</p><p>Thus, a holistic approach to the analysis of a plant extract consisting of two UHPSFC methods carried out on two columns and the same system without any manual intervention was developed and tested as a proof of concept. Indeed, most commercially available SFC instruments use a column manager that allows two or more columns to be connected simultaneously. Thus, it is still possible to analyze a complex sample in just two injections, taking advantage of the two stationary phases with different selectivity.</p><h4><strong>Application of UHPSFC-ESI/ESCi-MS/MS Method on Eucalyptus Extracts</strong></h4><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Analytical_Chemistry_Analytical_Chemistry_2024_96_7_2840_2848_Figure_4_Comparison_of_the_percentage_abundance_of_targeted_analytes_i_e_A_terpenes_B_terpenoic_acids_C_16211a715a.jpg" alt="Analytical Chemistry 2024 96 (7), 2840-2848: Figure 4. Comparison of the percentage abundance of targeted analytes, i.e., (A) terpenes, (B) terpenoic acids, (C).jpg"></p><h3><strong>Conclusions</strong></h3><p>UHPSFC-MS/MS is an interesting alternative to LC and GC methods, permitting the analysis of a wide range of compounds with a single instrument. Unfortunately, a single holistic method for the simultaneous analysis of terpenes and polar flavonoids remains unattainable due to two main challenges. No tested stationary phase enabled the retention and elution of both groups of analytes. However, new stationary phases are being introduced to the market every year, which is promising. Second, a universal ionization source combining GC and LC approaches is required for the simultaneous analysis of small lipophilic terpenes and polar glycosylated flavonoids.</p><p>Despite these challenges, we were able to develop a two-injection approach for complex plant analysis as a proof-of-concept based on the ability of the UHPSFC to cover supercritical, subcritical, enhanced-liquid, and liquid conditions within one instrument. Here, volatile terpenes are measured using a PGC stationary phase within supercritical to subcritical conditions achieved by adding up to 40% of MeOH to CO₂. More polar phenolic and terpenoic acids and flavonoids are then analyzed on short diol column with gradient from 0 to 90% MeOH with addition of 5% water.</p><p>The APCI source proved to be beneficial in the case of lipophilic volatiles when compared to ESI, but it was not possible to detect flavonoids using APCI. Conversely, US resulted in higher sensitivity for flavonoids, but similar to ESI, it was not possible to detect terpenes without hydroxy groups. The finally selected multimodal ESCi source was able to detect all targeted volatiles although the sensitivity was significantly lower than in the case of APCI. However, it was possible to switch from ESCi to ESI without any need for manual intervention, which was crucial for the applicability of the developed approach.</p><p>Finally, the quantitative aspects of the two developed UHPSFC-ESI/ESCi-MS/MS methods were determined, and the approach was successfully applied for the analysis of SFE extract from Eucalyptus sp. The novel approach can be beneficial for analysis of complex samples containing analytes with a wide range of physicochemical properties.</p>

Ultrahigh-Performance Supercritical Fluid Chromatography–Multimodal Ionization–Tandem Mass Spectrometry as a Universal Tool for the Analysis of Small Molecules in Complex Plant Extracts

<p><strong>In the week of August 12, the following webinars await you in the field of liquid phase and especially HPLC and LC/MS.</strong></p>
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<h4><a href="https://lcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4>
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<h5><strong>1. SelectScience/ Analytik Jena: Revolutionize drug discovery with high throughput mass spectrometry and automated pipetting</strong></h5>
<ul>
<li>Tu, 13.8.2024 17:00 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/4160">Registration</a></li>
</ul>
<p>The CyBio Well Vario pipetting device by Analytik Jena enhances MALDI spotting and sample optimization, seamlessly integrating with Bruker MS solutions to overcome application-specific bottlenecks.</p>
<h5><strong>2. Shimadzu Corporation: Elevating Pharma 4.0: Harnessing CaliberLIMS For Digital Excellence</strong></h5>
<ul>
<li>We, 14.8.2024 08:30 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/4163">Registration</a></li>
</ul>
<p>CaliberLIMS is a robust, scalable, and reliable platform designed to meet the demands of modern laboratories aiming for Pharma 4.0.</p>
<h5><strong>3. Waters Corporation: In-Line and On-Line Monitoring of CQAs for Biologics, Vaccines and Gene Vectors</strong></h5>
<ul>
<li>We, 14.8.2024 11:00 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/4176">Registration</a></li>
</ul>
<p>Principles, capabilities and limitations of RT-MALS, and then present case studies covering downstream processing of viral vectors, proteins, polysaccharides and lipid nanoparticles.</p>
<h5><strong>4. Metrohm: Accessing Battery Material Properties with Electrochemical Techniques</strong></h5>
<ul>
<li>We, 14.8.2024 17:00 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/4208">Registration</a></li>
</ul>
<p>This webinar will show examples of methodology, focusing on battery component properties such as the MacMullin number of separators, tortuosity of active material coatings, and electrolyte conductivity.</p>
<h5><strong>5. Agilent Technologies: Effective Use of Method EPA 8327/ASTM D8421/D8535 ‘Direct-Injection’ Techniques to Optimize Rapid TAT and Reduce Overall Project Costs</strong></h5>
<ul>
<li>We, 14.8.2024 17:00 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/4164">Registration</a></li>
</ul>
<p>Pace has developed and validated a ‘direct injection’ approach for PFAS analysis by LC-MS/MS, similar to the protocols described in EPA 8327 and ASTM D8421 &amp; D8535.</p>
<h5><strong>6. Waters Corporation: Multi-attribute quantitation of XDCs with Multi-Angle Light Scattering</strong></h5>
<ul>
<li>We, 14.8.2024 19:00 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/4162">Registration</a></li>
</ul>
<p>In this online seminar, we will demonstrate the value of light scattering in XDC development and its potential application in quality control (QC) as part of a release assay.</p>
<h5><strong>7. SCIEX: Whole blood microsampling methods for PFAS exposure biomonitoring</strong></h5>
<ul>
<li>We, 14.8.2024 19:00 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/3869">Registration</a></li>
</ul>
<p>Stay on the leading edge of all things PFAS with this enlightening monthly webinar series on testing workflows and cutting-edge technology that will demystify these “forever chemicals”.</p>
<h5><strong>8. Restek Corporation: Method Development Considerations for the LC-MS/MS Analysis of Drugs</strong></h5>
<ul>
<li>We, 14.8.2024 20:00 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/4184">Registration</a></li>
</ul>
<p>In this webinar, we will get you started on your analytical method with your column choice, including the particle, phase, and dimension.</p>
<h5><strong>9. Waters Corporation: Dietary Supplement Quality</strong></h5>
<ul>
<li>Th, 15.8.2024 19:00 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/4167">Registration</a></li>
</ul>
<p>Solving Problems That Matter - a Waters webinar series featuring USP speakers. Episode 7: Dietary Supplement Quality</p>
<h5><strong>10. Agilent Technologies: UV-VIS-NIR in Battery Development</strong></h5>
<ul>
<li>Th, 15.8.2024 20:00 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/3909">Registration</a></li>
</ul>
<p>Agilent&#39;s portfolio of instruments offers the high performance and flexible accessories needed for pioneering new applications.</p>


Webinars LabRulezLCMS Week 33/2024

<p><strong>In the 2 weeks from August 12, the following webinars await you in the field of atomic and molecular spectroscopy and spectrometry</strong></p>
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<h4><a href="https://icpms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4>
</blockquote>
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<p><strong>👉 Search and filter in the largest global database</strong>  with over <strong>3 500 GC, LC, MS and spectroscopy webinars</strong>.</p>
</blockquote>
<h5><strong>1. Shimadzu Corporation: Elevating Pharma 4.0: Harnessing CaliberLIMS For Digital Excellence</strong></h5>
<ul>
<li>We, 14.8.2024 08:30 CEST</li>
<li><a href="https://icpms.labrulez.com/webinar/4163">Registration</a></li>
</ul>
<p>CaliberLIMS is a robust, scalable, and reliable platform designed to meet the demands of modern laboratories aiming for Pharma 4.0.</p>
<h5><strong>2. Thermo Fisher Scientific: Dealing with the Complexity of High Matrix Samples on ICP-OES and ICP-MS</strong></h5>
<ul>
<li>We, 14.8.2024 13:00 CEST</li>
<li><a href="https://icpms.labrulez.com/webinar/4193">Registration</a></li>
</ul>
<p>Techniques available to deal with these samples.</p>
<h5><strong>3. Agilent Technologies: UV-VIS-NIR in Battery Development</strong></h5>
<ul>
<li>We, 15.8.2024 20:00 CEST</li>
<li><a href="https://icpms.labrulez.com/webinar/3909">Registration</a></li>
</ul>
<p>Agilent&#39;s portfolio of instruments offers the high performance and flexible accessories needed for pioneering new applications.</p>
<h5><strong>4. SelectScience/CYTEK: Improving Results Through Better Understanding: A Primer On High-Dimensional Flow Cytometry Technologies And Reagents</strong></h5>
<ul>
<li>Tu, 20.8.2024 17:00 CEST</li>
<li><a href="https://icpms.labrulez.com/webinar/4186">Registration</a></li>
</ul>
<p>A broad overview of available high-dimensional flow cytometry technologies and reagents, how they work, and an experience-informed breakdown of the strengths and limitations of each technique. </p>
<h5><strong>5. Agilent Technologies: Analysis of Electrolyte and Li salts commonly used in Li Battery manufacturing</strong></h5>
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<li>Tu, 20.8.2024 21:30 CEST</li>
<li><a href="https://icpms.labrulez.com/webinar/3910">Registration</a></li>
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<p>Analysis of Electrolyte and Li salts commonly used in Li Battery manufacturing.</p>
<h5><strong>6. Agilent Technologies: The benefits of a fully Integrated Advanced Dilution System (ADS) for ICP-OES</strong></h5>
<ul>
<li>Th, 22.8.2024 20:00 CEST</li>
<li><a href="https://icpms.labrulez.com/webinar/3911">Registration</a></li>
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<p>Boost productivity and eliminate tedious standard and sample preparation using Agilent’s Advanced Dilution System (ADS) with the ICP-OES.</p>


Webinars LabRulezICPMS Week 33-34/2024

A comparison of sensory evaluation and an electronic nose assay in the assessment of aroma in dry hopped beers

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 5th August 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p>
<blockquote>
<h4>👉 <a href="https://gcms.labrulez.com/library"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></a></h4>
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</blockquote>
<p>This week we bring to you applications and other documents by <strong>LECO</strong>, <strong>Agilent Technologies</strong>, <strong>Waters Corporation</strong>, and <strong>Shimadzu</strong>!</p>
<h4><strong>1. LECO: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Essential_Oil_Fragrance_Samples_BT_G_Cx_GC_Paradigm_Shift_SA_CK_ANALYTIKA_SA_24_LPSS_318_8458df1480.pdf">Non-Target Characterization of Complex Essential Oil and Fragrance Samples with GCxGC-MS/FID for Reliable Identification and Relative Quantitation in a Single Injection</a></strong></h4>
<ul>
<li>poster / Analytica</li>
</ul>
<p><strong>Introduction:</strong> Essential oils are extracts from plant materials that capture the plant&#39;s scent and flavors. They have a broad range of applications, as they can be both a finished product and an ingredient or intermediate in the creation of other products. Due to this versatility, the analysis of essential oils is an important area of research with a variety of analytical objectives. </p>
<p>Because flavors and fragrances are composed of tens or hundreds of ingredients, characterization of these individual species can be challenging. It is not practical to use numerous standards for the identification and quantification of all the individual species. Instead, it is common to use a workflow where MS provides identification and FID provides relative area % quantification, often with separate injections for each.</p>
<p>Additionally, two one-dimensional chromatographic separations with different stationary phases are also often required to isolate the individual compounds due to the complexity of these samples. Here, we demonstrate a possible improvement to this workflow by using a GCxGC-TOFMS/FID instrument that provides reliable identification and relative quantitation in a single injection. GCxGC provides enhanced chromatographic separation of individual analytes, thus removing the requirement for two separate 1D analyses. Coupling this with dual MS and FID detection enables both identification via the FID in one single injection.</p>
<p><strong>Conclusion:</strong> Harnessing the power of a TOFMS coupled with a GCxGC platform and an FID allowed us to not only determine the presence and amounts of targeted analytes, but also discover non-target analytes.</p>
<p>This platform, based on GCxGC-TOFMS/FID, can improve workflows in your industry.</p>
<h4><strong>2. Shimadzu: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00788_en_8355bce383.pdf">Comprehensive Characterization of Diesel Fuel on GC×GC Utilizing Impressive High-Speed Scan Technology of GCMS-QP2050</a></strong></h4>
<ul>
<li>Application</li>
</ul>
<p><strong>User Benefits</strong></p>
<ul>
<li>Comprehensive characterization of complex matrices such as diesel fuel is possible with 2D gas chromatography.</li>
<li>The impressive high-speed scan technology of GCMS-QP2050 allows for effective peak separation.</li>
<li>Intuitive comprehension of compounds distribution can be achieved with displaying the data in a two-dimensional image.</li>
</ul>
<p><strong>Introduction:</strong> Kerosene, diesel, and other petroleum products are mixtures containing over 100 different hydrocarbons. The properties of petroleum products, such as ignitability and viscosity, depend on their composition and greatly affect physical properties like combustion. Comprehensive two-dimensional gas chromatography (GC×GC) offers high separation performance by utilizing two different columns, which provides more reliable compositional information for complex mixtures compared to one-dimensional chromatography. In this application, qualitative analysis of diesel fuel using a GC×GC system with GCMS-QP2050 that is capable of high-speed scanning (30,000 u/sec) was conducted. No less than 30,000 u/sec scanning speed improved the separation of peaks that are too close to each other and enabled accurate identification of compounds.</p>
<p><strong>Conclusion:</strong> Diesel, a complex mixture of hydrocarbons, was measured using GC×GC-MS. Each component on the two-dimensional image showed characteristic distribution based on its molecular structure, allowing for intuitively understanding of the composition of diesel. Additionally, GC×GC-MS demonstrated Excellentseparation performance for components, enabling more reliable identification of components of diesel compared to 1D GC-MS. The high-speed scan of GCMS-QP2050 (30,000 u/sec) contributesto more precise qualification analysis.</p>
<h4><strong>3. Shimadzu: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_05_sca_280_108_en_d87677c8a2.pdf">Analysis of Trialkyl Phosphates as Markers for Lithium Battery Aging</a></strong></h4>
<ul>
<li>Application</li>
</ul>
<p><strong>User Benefits</strong></p>
<ul>
<li>Lithium Batteries(LIB) decomposition and aging can be evaluated by monitoring Trialkyl Phosphates.</li>
<li>A routine and fast GCMS method for the detection of Trialkyl Phosphates was developed.</li>
<li>Trialkyl Phosphates can be detected with high sensitivity and selectivity in commercial liquid electrolytes</li>
</ul>
<p><strong>Introduction:</strong> The electrolyte solution is a crucial part of a typical Lithium-ion battery, consisting of Li salts (e.g. LiPF6), and organic carbonates. Decomposition and formation of phosphorous-based and other organic products starts already at the production stage of the electrolyte. The formation of such molecules does not affect the electrolyte/battery quality negatively, as long as the quantity is low enough. On the contrary, several decomposition products have a positive effect on the formation of the so-called SEI surface (Solid Electrolyte Interface) on the LIB anodes, which is crucial for the battery functionality. Nevertheless, this is a continuous chemical process and the increasing amount of some of the decomposition products is a clear indicator of the progressive aging of the battery/electrolyte. This application is demonstrating the GCMS analysis of Trialkyl Phosphates as reaction products of carbonates and LiPF6 salt. The choice of this compounds as markers for electrochemical battery aging is due to the fact, that their formation is very slow and depends only on a few external parameters, allowing to investigate the electrochemical aging (charge/discharge) by a simple comparison of before/after analyte content.</p>
<p><strong>Conclusion:</strong> The presented application demonstrated the suitability of GCMS to investigate the aging of the LIBs using phosphatebased degradation products. This investigation is based on SCAN measurements. Here, a SCAN/SIM mode would be beneficial offering the possibility to detect the main compounds (carbonated, additives) and the degradation products in one measurement. A further improvement would be a dedicated SIM method for the mentioned phosphates with the highest selectivity and sensitivity.</p>
<h4><strong>4. Agilent Technologies: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_dithiocarbamate_pesticide_tea_gc_5994_7663en_agilent_78da56d0be.pdf">Analysis of Dithiocarbamate Pesticides in Tea Using GC/MS/MS</a></strong></h4>
<ul>
<li>Application Note -Food Testing and Agriculture</li>
</ul>
<p><strong>Abstract:</strong> Dithiocarbamate pesticides are commonly used to control fungal diseases in ornamental plants and crops, and for control of tea gray blight. The residue definition for dithiocarbamate pesticides is expressed as total dithiocarbamate, determined as mg CS₂/kg. Methods for analysis of CS₂ use extraction of the sample into an acidified stannous chloride solution with isooctane, where the dithiocarbamate residues are converted to CS₂, which is captured in isooctane and analyzed by GC/MS. This application note describes the analysis of dithiocarbamate residues in tea using an Agilent GC/MS/MS in both SIM and MRM modes. A limit of quantification of 10 ppb was achieved in tea samples. Linearity was established in matrix-matched standards with R2 &gt; 0.999 for the range from 5 to 100 ppb, with average recoveries &gt; 85% at the 10 ppb level of fortification.</p>
<p><strong>Conclusion:</strong> Analysis of dithiocarbamate pesticides as CS₂, using isooctane as a sample preparation solvent, can lead to the combination of a relatively high boiling solvent with low boiling analytes. Hot spitless injections result in poor peak shapes for CS₂; better peak shapes can be obtained with cold injection in split mode. Further improvement in peak shapes can be achieved by using a multibaffled liner. Matrixmatched calibration standards ranging from 5 to 100 ppb were used to assess calibration performance, with linearity established at R² &gt; 0.999 in both SIM and MS/MS modes. The method was validated following the criteria specified in SANTE 11312/2021v2, with the ability to detect CS₂ peaks down to 5 ppb using Agilent 7000D, 7000E, and 7010C GC/MS/MS instruments. Implementing a backflush method in the GC/MS analysis of tea samples can significantly improve the separation of target analytes from complex matrix components, enhancing sensitivity and throughput. Repeatability tests showed RSDs consistently below 4.2% for injections at 10 ppb concentration, indicating high precision and repeatability </p>
<h4><strong>5. Waters Corporation: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008300_en_1dd7d73213.pdf">Converting Target Analysis of Organochlorine Pesticides in Environmental Matrices from Electron Ionization GC-HRMS Using Helium Carrier Gas to Atmospheric Pressure Ionization GC-MS/MS Using Nitrogen Carrier Gas</a></strong></h4>
<ul>
<li>Application Note</li>
</ul>
<p><strong>Abstract:</strong> Organochlorine pesticides (OCPs) are among the high production volume chemicals produced in the past that had wide application and exhibit significant persistence in the environment. DDT, for example, has a half-life in sediment of up to 15 years meaning that it may not be 90% degraded for 45 to 60 years.¹ Furthermore, they are associated with a number of negative health effects when bioaccumulated in humans and animals. These are among the reasons that nine of the initial 12 compounds addressed by the 2004 Stockholm Convention on Persistent Organic Pollutants (POPs) belong to this compound class.² </p>
<p>Due to the complexity of matrices, such as sediment and biota, encountered when monitoring the fate, transportand occurrence of these compounds, it is necessary to employ techniques with high sensitivity, specificity, and robustness for these studies. In the past this has required the use of complex sample extraction and clean-up combined with electron ionization (EI) and high resolution mass spectrometry (HRMS) using magnetic sector instrumentation. However, in recent years the performance of Gas Chromatography Atmospheric Pressure Ionization Tandem Quadrupole Mass Spectrometry (GC-APCI-MS/MS) has demonstrated equal or better performance than the classic technique.³ In this work the Atmospheric Pressure Gas Chromatography (APGC™) ionization source on a Xevo™ TQ-XS Tandem Quadrupole System was used with both helium (He) and nitrogen (N₂) carrier gas to analyze sediment and biota extracts for the presence of 39 OCPs. Performance characteristics and sample quantification results for APGC-MS/MS were compared with results for the same aliquots run using GC-EI-HRMS.</p>
<p><strong>Conclusion:</strong> The GC-EI-HRMS reference method separations and runtime were matched on the APGC-MS/MS system with only minor modification to the He carrier gas flowrate. Scaling of the column dimensions for use with N₂ carrier gas effectively reproduced the reference method separations and total runtime which allows the use of the same acquisition and processing files across both configurations. The comparison between the APGC He and N₂ carrier gas data shows that sensitivity is also maintained within a factor of two times between the two carrier gases. Analysis of extracted samples of biota and sediment indicate good agreement between the APGC N₂ carrier gas method and the EI HRMS reference method values. These results demonstrate the feasibility of modernizing the traditional reference method with a technique that is more easily integrated into most labs and more accessible for most operators.</p>


News from LabRulezGCMS Library - Week 32, 2024

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 5th August 2024? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p>
<blockquote>
<h4>👉 <a href="https://lcms.labrulez.com/library"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></a></h4>
</blockquote>
<blockquote>
<p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p>
</blockquote>
<p>This week we bring to you applications, brochures and specifications from <strong>Agilent Technologies</strong>, <strong>Shimadzu</strong>, <strong>Metrohm</strong>, <strong>Thermo Fisher Scientific,</strong> and <strong>Waters Corporation</strong>!</p>
<h4><strong>1. Shimadzu: <a href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/IVDR_White_Paper_2024_Shimadzu_737d95b5fb.pdf">How Shimadzu is simplifying your compliance workload for the new IVD regulation!</a></strong></h4>
<ul>
<li>Technical Note</li>
</ul>
<p><strong>What is the New EU In Vitro Diagnostic Regulation (IVDR)?</strong></p>
<p>New In Vitro Diagnostic Medical Device Regulation (IVDR) (EU) 2017/746 was published in EU Official Journal in May 2017 in order to ensure a high level of safety and health whilst supporting innovation. It applies from 26 May 2022 and replaced the previous IVD Directive (98/79/EC). This regulation set rules for in vitro diagnostic devices such as reagent, calibrator, kit, instrument, and software intended by the manufacturer to be used for diagnostic purposes.</p>
<p>IVDR retains some concepts of IVD Directive such as CE marking or essential requirements (under IVDR called “general safety and performance requirements”). As in the past, the manufacturers have to demonstrate that they and their devices meet the requirements through conformity assessment procedure.</p>
<p>Different from IVD Directive, however, IVDR introduced the riskbased classification (Figure 1). Under IVDR devices are classified in four: The devices with highest risks are classified in class D. The class A devices have low risks and include products for general laboratory use, accessories which possess no critical characteristics.</p>
<h4><strong>2. Shimadzu: <a href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/LCMS_157_Determination_of_30_PFAS_Seafood_LCMS_8060_NX_060524_a44e3a68b5.pdf">Determination of 30 PFAS in Seafood by Liquid Chromatography Triple Quadrupole Mass Spectrometry (LC-MS/MS)</a></strong></h4>
<ul>
<li>Application</li>
</ul>
<p><strong>User Benefits</strong></p>
<ul>
<li>Validated method for 30 PFAS in seafood (shrimp) meeting all criteria of AOAC SMPR 2023.003</li>
<li>High precision, excellent recovery, low Limit of Quantification (LOQ)</li>
<li>Simple and rapid extraction using QuEChERS</li>
</ul>
<p><strong>Introduction:</strong> Per-and polyfluorinated substances (PFAS) are a diverse group of man-made chemicals used in numerous products since the 1950s. PFAS can enter the food supply by contact in environmentally contaminated areas, during food processing, or exposure to packaging. Because PFAS have been linked to serious health effects, accurate methodology is needed. In this application news, we describe a single laboratory validation study with a rapid extraction of low concentrations of 30 PFAS in shrimp using the QuEChERS technique followed by analysis using the Shimadzu Nexera Liquid Chromatograph coupled to a Shimadzu LCMS-8060NX triple quadrupole mass spectrometer (Figure 1). </p>
<p>We optimized the chromatography and instrument operating parameters to achieve excellent peak shape, separation, and sensitivity. Sensitivity was improved for 4  PFAS, PFOA, PFHxS, PFNA, and PFOS.</p>
<p>In this study, we spiked samples at three concentrations in triplicate. For greater accuracy, standards were matrixmatched and extracted and spikes were quantified using the isotope dilution technique. Recovery and precision were compared to the requirements of AOAC SMPR 2023.003. In addition, we determined the Limit of Quantitation (LOQ) as the lowest concentration meeting accuracy and precision, ion ratio, retention time, and signal-to-noise ratio criteria of the qualifier ion. All recovery, precision, and LOQ’s met the acceptance criteria of the SMPR. The target analytes, their acronym, chemical abstract number, and experimentally determined LOQ are shown in Table 1.</p>
<p><strong>Conclusion:</strong> The Shimadzu LCMS-8060NX Triple Quadrupole Mass Spectrometer coupled with a Shimadzu Nexera Liquid Chromatograph was used in a single laboratory study to measure 30 PFAS compounds in a shrimp matrix and compared to criteria set by AOAC SMPR 2023.003. Chromatography conditions and the mass spectrometer were optimized to achieve excellent separation of all analytes, baseline resolution between linear and branched isomers, and a two-minute separation between PFOS and potentially interfering cholic acids. </p>
<p>Precision and recovery and the experimentally determined LOQ are well within the requirements of the SMPR.</p>
<h4><strong>3. Agilent Technologies: <a href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/technical_overview_lc_ms_intelligence_5994_7430en_agilent_b00bf96408.pdf">Boost Efficiency and Productivity with Instrument Intelligence and Workflow Automation</a></strong></h4>
<ul>
<li>Technical Note</li>
</ul>
<p><strong>Introduction:</strong> Ever-increasing pressure for laboratories to minimize operating costs while maximizing output demands innovative approaches to their daily work. Recent developments in artificial intelligence (AI) and automation can help to alleviate this growing burden. The goal is to get technology to contribute more and more to day-to-day operations by reducing errors and ensuring consistent high-quality data generation. For workflows using Agilent LC/TQ and LC/(Q-)TOF instruments, this goal is becoming a reality.</p>
<p>The latest generation of Agilent LC/TQ and LC/(Q-)TOF instruments offers a suite of intelligent automation features to keep the instruments at peak performance. SWARM autotune allows instruments to be tuned for specific applications and desired performance. Auto- and check tunes can be scheduled to run during downtime so that the instruments are always ready to go. Instrument status is actively monitored using Early Maintenance Feedback (EMF) with constant feedback so that users can anticipate and plan for maintenance. Data are actively examined to ensure high quality. And, if data-related issues are suspected, Intelligent Reflex reinjection workflows automatically work to correct the situation. The culmination of these instrument intelligence features reduces errors, rework, and manual intervention—boosting laboratory efficiency and productivity.</p>
<p><strong>Conclusion:</strong> Agilent LC/TQ and LC/(Q-)TOF instruments include numerous intelligence and workflow automation features to boost productivity and efficiency of demanding routine analysis applications. These intelligence features:</p>
<ul>
<li>Maximize instrument performance and analytical sensitivity (application-based SWARM autotune)</li>
<li>Minimize downtime (early maintenance feedback and scheduled tuning)</li>
<li>Maximize sample throughput (intelligent reflex and fast screening workflows) </li>
<li>Ensure that injected samples do not require repeat work(intelligent reflex carryover detection and above calibration range workflows)</li>
<li>Improve sample characterization (intelligent reflex targeted MS/MS confirmation and iterative MS/MS workflows)</li>
</ul>
<h4><strong>4. Agilent Technologies: <a href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_peptide_impurity_two_dimensional_liquid_chromatograhy_5994_7654en_agilent_e71c92f265.pdf">Confirmation of Peptide-Related Impurity Intact Mass Using Agilent 1290 Infinity II Bio 2D-LC and InfinityLab LC/MSD XT</a></strong></h4>
<ul>
<li>Application</li>
</ul>
<p><strong>Abstract:</strong> This application note presents the analysis of peptide-related impurities for Semaglutide using an Agilent 1290 Infinity II bio 2D-LC and an Agilent InfinityLab LC/MSD XT system. Peptide-related impurities are challenging to separate from peptide-active pharmaceutical ingredients due to their structural diversity and relatively large molecular weights. To address this challenge, an Agilent AdvanceBio Peptide Plus column, which is stable under high-concentration acidic conditions, was used to achieve good separation of Semaglutide impurities. A solvent system compatible with mass spectrometry (MS) was used with the 1290 Infinity II bio 2D-LC and InfinityLab LC/MSD XT, enabling the acquisition of MS spectra. The deconvolution feature in Agilent OpenLab CDS software, version 2.8, facilitated the easy determination of molecular weights for impurity peaks analyzed by two-dimensional liquid chromatography (2D-LC).</p>
<p><strong>Conclusion:</strong> Generally, difficult-to-separate peptide-related impurities can benefit from improved resolution through optimizing the concentration of acidic modifiers and fine-tuning the column performance. However, confirming the molecular weight of impurities can be challenging due to mobile phases not being suitable for MS analysis. In this application note, a stability indicating test for Semaglutide demonstrated efficient transition to LC conditions compatible with MS analysis using the Agilent InfinityLab multiple heart-cutting valve feature of an Agilent 1290 Infinity II bio 2D-LC. An Agilent InfinityLab LC/MSD XT exhibited the sensitivity to confirm MS spectra, even when analyzing impurities at low concentrations in the second dimension, and the deconvolution feature of Agilent OpenLab CDS software, version 2.8, facilitated easy confirmation of accurate molecular weights. Based on these results, it is anticipated that this method will provide foundational data for the management of peptide-related impurities not only for formulation compatibility but also for stability studies.</p>
<h4><strong>5. Thermo Fisher Scientific: <a href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/fl_002789_ccs_dnapac_rp_columns_fl002789_en_6747763b83.pdf">Revolutionize your oligonucleotide analysis with game-changing DNAPac RP columns</a></strong></h4>
<ul>
<li>Other</li>
</ul>
<p><strong>The semi-preparative format –  ideal for nucleic acid purification</strong></p>
<p>Product features</p>
<ul>
<li>Designed for ion-pair reversed-phase (IP-RP) LC and  LC/MS separations of both single-stranded oligonucleotides  and double-stranded nucleic acids</li>
<li>Unique selectivity of the DNAPac RP chemistry, now available  for puriﬁcation</li>
<li>Bioinert hardware to eliminate analyte adsorption and avoid  the need for column passivation</li>
<li>Wide operating pH range and high-temperature stability  (up to 110 °C)</li>
<li>High resolution and high throughput</li>
</ul>
<h4><strong>6. Thermo Fisher Scientific: <a href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/fl_22070_dnapac_dnaswift_oligonucleotide_fl22070_en_99e4d8f460.pdf">Thermo Scientific DNAPac columns - Ultra-high resolution oligonucleotide separation</a></strong></h4>
<ul>
<li><p>Other</p>
</li>
<li><p><strong>Thermo Scientiﬁc™ DNAPac™ PA200 and DNAPac™ PA200RS Columns</strong> oﬀer the highest resolution charge based  oligonucleotide separations. These anion-exchange columns  provide unsurpassed resolution of full length from n–1, n+1 (and  other failure sequences). </p>
</li>
<li><p><strong>Thermo Scientiﬁc™ DNAPac™ RP (U)HPLC Columns</strong> are high-throughput, high-resolution columns designed for  ion-pair reversed-phase separations. They are compatible  with LC-MS, have long-lasting polymeric columns, and  can operate up to pH 14. They also have temperature  stability up to 110 °C. These columns can easily resolve  both small polynucleotides and large dsDNA fragments  up to 10,000 bp due to pores varying from 50-2000Å.  Now available in semi-preparative format.</p>
</li>
<li><p><strong>Thermo Scientiﬁc™ DNASwift™ SAX-1S Monolith Column</strong> provide high loading capacity for easy laboratory scale  charge-based puriﬁcation of oligonucleotide samples.</p>
</li>
</ul>
<h4><strong>7. Waters Corporation: <a href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/fl_22070_dnapac_dnaswift_oligonucleotide_fl22070_en_99e4d8f460.pdf">VISUALIZATION AND QUANTIFICATION OF DRUG/METABOLITES BY SENSITIVE AND FAST TARGETED DESI IMAGING ON TQ SYSTEM</a></strong></h4>
<ul>
<li>Poster / <a href="https://lcms.labrulez.com/events/568"><strong>ASMS 2024</strong></a></li>
</ul>
<p><strong>INTRODUCTION:</strong> Mass spectrometry (MS) coupled to liquid chromatography (LC) has been typically used for drug metabolism and pharmacokinetics (DMPK) studies. However, tissues are homogenised and therefore the molecular localisation is lost.</p>
<p>Desorption electrospray ionization (DESI) mass  spectrometry imaging (MSI) has proven to successfully  map and independently quantify small molecules without  radioactive labelling. Including small pharmaceutical  molecules, as well as endogenous metabolites directly  from tissue without the need of sample preparation after  sectioning.</p>
<p>Tandem quadrupole (TQ) MS are renowned for their  sensitivity and specificity in targeted applications using  Multiple reaction monitoring (MRM) mode of acquisition.</p>
<p>Here, we used a commercial central nervous system  (CNS) active drug named pitolisant that treats  narcolepsy. It was dosed at pharmacological level and no  observed adverse effect level (NOAEL) to show the  distribution of the drug and its main metabolite in  different organs such as liver and brain using the  sensitive and fast DESI TQ system.</p>
<p><strong>CONCLUSION</strong></p>
<ul>
<li>Pitolisant and its metabolites were detected sub 0.1 ng  when spotted onto tissue section, demonstrating the  high sensitivity and specificity of targeted MRM MS  Imaging workflow.</li>
<li>A highly flexibility workflow is evidenced allowing high  speed DESI MSI experiments with no compromise in  sensitivity or including more MRM transitions to map  biomarkers as well as drug.</li>
<li>Pitolisant and its oxidized metabolite were easily  detected at pharmacological dose, illustrating the  different distributions in the liver and brain murine  tissue sections, information that wouldn’t be  discovered by traditional DMPK studies.</li>
<li>MSI quantification workflow is demonstrated with the  in-house MicroApp MSI Quantify.</li>
</ul>
<h4><strong>8. Waters Corporation: <a href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/2024_asms_claude_q_tof_ae3ec65164.pdf">EVALUATION OF DESI MOUNTED ON Q-TOF AND TQ MASS SPECTROMETERS TO IMAGE PFAS COMPOUNDS IN DIFFERENT MATRICES</a></strong></h4>
<ul>
<li>Poster / <a href="https://lcms.labrulez.com/events/568"><strong>ASMS 2024</strong></a></li>
</ul>
<p><strong>INTRODUCTION:</strong> Per- and polyfluoroalkyl substances (PFAS) are a well-  known group of chemicals that have a variety of  commercial and consumer uses. They have been found  to be highly persistent and can accumulate in humans,  animals and the environment.</p>
<p>Traditionally, analysis of PFAS has focused on  determination with LC-MS/MS. Often laborious SPE  techniques are required before analysis of solid matrices,  such as food, plants or animal tissue to assess exposure  routes. Furthermore, samples are homogenized, and  therefore the information of where the PFAS accumulate  is not available.</p>
<p>Here we evaluate mass spectrometry imaging (MSI) to  detect PFAS directly from sample surfaces.  Figure 5. Multiple conformations of N-EtFOSAA and corresponding spe-  cific drift time ion images of the dilution series. Analyzed using SE-  LECT SERIES Cyclic IMS MS in IMS mode .  A desorption electrospray ionization (DESI) source  combined with two types of Q-Tof mass spectrometers  operating in full scan MS (with and without, and a high  performance tandem quadrupole mass spectrometer  operating in targeted multiple reaction monitoring (MRM)  mode were used to evaluate limits of detection (LODs) of  several PFAS compounds.</p>
<p><strong>CONCLUSION</strong></p>
<ul>
<li>61% and 55% of the PFAS compounds were detected as low as  10 ng/mL spotted on tissue when analyzed by negative mode  DESI in discovery full scan MS acquisition mode.</li>
<li>The targeted MRM acquisition mode on the DESI XS Xevo TQ  Absolute MS is the most sensitive system with 77% of the PFAS  compounds detected as low as 10 ng/mL spotted on tissue.</li>
<li>PFAS compounds have a different ion mobility, with faster  arrival time in the gas phase, allowing differential selection and  a decrease of interference signal.</li>
<li>Different conformations of several PFAS were detected by ion  mobility with only a single pass in the cyclic device.</li>
<li>Distinct distributions of PFAS in the seed and root of  contaminated PFAS lentils were demonstrated.</li>
</ul>
<h4><strong>9. Metrohm: <a href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_eis_009_download_1f476a3249.pdf">Mott-Schottky Analysis - Using EIS for semiconductor applications</a></strong></h4>
<ul>
<li>Application</li>
</ul>
<p><strong>Using EIS for semiconductor applications:</strong> Semiconductors are intrinsic to modern life, but they stand to play an even greater role in the coming energy transition. Several techniques are employed in the pursuit of improved materials for energy production and storage. One particularly popular method for studying the electronic properties of potential new semiconducting materials is MottSchottky Analysis. The technique can be best understood as an extension of electrochemical impedance spectroscopy (EIS). By performing EIS at a range of different DC bias or offset potentials, the reciprocal of the square capacitance can be derived from the data and then plotted against the DC offset itself, producing a so-called Mott-Schottky Plot. From such a plot, critical parameters such as the carrier concentration, the doping profile, and the flatband potential can be conveniently extracted. This technique is popular across different fields, as it is versatile, non-destructive, and relatively fast. Compared to other options, Mott-Schottky Analysis also requires relatively little specialist equipment. This Application Note presents an example of MottSchottky measurement on a popular semiconducting material using VIONIC powered by INTELLO.</p>
<p><strong>CONCLUSIONS:</strong> In this Application Note, an example Mott-Schottky measurement is shown using VIONIC powered by INTELLO. The flatband potential and doping density have been calculated using NOVA and are comparable to values for this type of sample found in the literature.</p>


News from LabRulezLCMS Library - Week 32, 2024

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week 32, 2024? Check out new documents from the field of spectroscopy, especially ICP/MS techniques!</strong></p>
<blockquote>
<h4>👉 <a href="https://icpms.labrulez.com/library"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT ICPMS AND RELATED TECHNIQUES</strong></a></h4>
</blockquote>
<blockquote>
<p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> libraries.</p>
</blockquote>
<h4><strong>1. Metrohm: <a href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Metrohm_OMNIS_NIRS_An_efficiency_boost_for_your_706048fea4.pdf">OMNIS NIRS: An efficiency boost for your laboratory</a></strong></h4>
<ul>
<li>Technical note</li>
</ul>
<p><strong>Routine lab analysis – simplified with OMNIS NIRS</strong></p>
<p>Near-infrared spectroscopy (NIRS) is an analytical technique used to determine multiple parameters in samples quickly without requiring any chemicals. Determinations can be performed in liquids, pastes, and solids with this non-destructive method.</p>
<p>Many industries benefit from using NIRS in their laboratory workflows. Time and cost savings are two of the most convincing arguments for adopting NIRS in the laboratory. It is also easy to use, even for non-technical operators.</p>
<p>This White Paper discusses the concept and benefits of NIR spectroscopy, supplemented with the use of the Metrohm NIR solution, OMNIS NIRS, in several real-life laboratory application examples. Applications from the <strong>petrochemical</strong>, <strong>food and beverage</strong>, <strong>semiconductor</strong>, and** pharmaceutical industries** are used to demonstrate the unique functionalities of OMNIS NIRS in different situations.</p>
<p><strong>SUMMARY</strong></p>
<p>With OMNIS NIRS, users get a flexible, modular analytical solution which is suitable for many industries. Unique functionalities include:</p>
<ul>
<li>automatic model development (OMD)</li>
<li>a high measurement speed</li>
<li>the possibility to recognize sample insertion and removal</li>
<li>sophisticated temperature control</li>
<li>the ability to combine different analytical technologies from a single manufacturer - even in an automated system</li>
</ul>
<p>Boost the efficiency of your laboratory with OMNIS NIRS.</p>
<h4><strong>2. Thermo Fisher Scientific: <a href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_002821_tea_icap_ms_icap_tqe_industrial_an002821_em_en_b60acdccc6.pdf">Analysis of process water from hydrogen fuel cells using triple quadrupole inductively coupled plasma mass spectrometry (ICP-MS)</a></strong></h4>
<ul>
<li>Application</li>
</ul>
<p><strong>Goal:</strong> To demonstrate the analysis of process water from hydrogen fuel cells for inorganic trace contaminants with high sensitivity and accuracy using triple quadrupole ICP-MS.</p>
<p><strong>Keywords:</strong>  Fluorine, fuel cell, high resolution, ICP-MS, KED, PEM, process water, triple quadrupole, TQ-O2 mode</p>
<p><strong>Conclusions:</strong> The iCAP TQe ICP-MS was employed to analyze 53 elements including fluorine in process water derived from hydrogen fuel cells. Among the analytes, several critical interferences can cause unexpected bias, and these were investigated closely for effective and complete removal by means of selective collision / reaction cell reactions with oxygen. This study also included the development of a method for the analysis of fluorine, generally only possible in an indirect measurement. This analytical method was rigorously tested, and the results obtained clearly demonstrate the fowling analytical advantages:</p>
<ul>
<li>The iCAP TQe ICP-MS operated in TQ-O2 and He KED modes allowed the analysis of 53 elements in relevant sample matrices over a wide concentration range. For minor elements, the method was tested over 4 orders of magnitude (from 0.01 to 100 µg·L-1), whereas major elements were tested between 1 to 100 µg·L-1.</li>
<li>Using a high throughput analysis approach, with a new autosampler equipped with a Step Ahead feature for minimizing total analysis time, all elements relevant for the development of hydrogen fuel cell technology could be measured accurately with low detection limits.</li>
<li>The use of TQ-O₂ mode provided advanced performance for eliminating the polyatomic interferences of phosphorus, sulfur, silver, and cadmium in the simulated hydrogen fuel cell process water. This covered both polyatomic interferences as well as overlaps created by intense signals from isotopes of elements present in high concentrations.</li>
<li>The iCAP TQe ICP-MS offers the flexibility to choose high resolution for the Q1 and Q3 quadrupoles, enabling complete elimination of polyatomic interference and isobaric interferences. </li>
<li>The feasibility of fluorine analysis was demonstrated using an indirect method after complexation with barium. The iCAP TQe ICP-MS showed accurate and precise determination of fluorine as proven by the spike recovery tests performed.</li>
<li>Excellent stability performance was obtained with the iCAP TQe ICP-MS together with excellent CCV and spike recovery results over a 3-hour run without internal standard correction. This provides the advantage of avoiding potential contamination from addition of the internal standard solution.</li>
</ul>
<h4><strong>3. Thermo Fisher Scientific: <a href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an41218_oe_basic_inclusion_analysis_en_024ffa9f51.pdf">Iron and steel - ARL iSpark Plus Optical Emission Spectrometer</a></strong></h4>
<ul>
<li>Application</li>
</ul>
<p><strong>Basic inclusion analysis</strong></p>
<p>Non-metallic inclusions dramatically affect steel properties and cause process issues like nozzle clogging. The costs associated with bad steel properties, process issues or customer complaints may amount to several hundred thousand dollars every year. Controlling the formation and the modification of non-metallic inclusions has therefore become essential to the production of modern steels as demanded by today’s markets.</p>
<p>The Thermo Scientific ARL iSpark Plus is a high-end metal analyzer that allows precise and accurate elemental analysis of steel. It also enables ultra-fast analysis of non-metallic inclusions, enabling a steel plant to control steel quality and production process even more effectively, and considerably reduce the costs associated with unwanted inclusions.</p>
<p>The Basic Inclusion Analysis Spark-DAT (Spark Data Analysis and Treatment) option is the entry-level method for standard inclusion analysis in low alloy steel. It reports the amounts of some of the most common types of non-metallic inclusions together with the elemental concentrations, helping steel plants to guarantee the quality and the properties of the steel product, as well as the smooth running of the production process.</p>
<p><strong>Benefits</strong></p>
<ul>
<li>Ultra-fast evaluation of some main inclusion types</li>
<li>Close to real-time inclusion check in up to hundreds of samples a day</li>
<li>More effective control of inclusiondependent steel properties</li>
<li>Helps reduce the number of costly issues caused by inclusions</li>
</ul>
<h4><strong>4. Agilent Technologies: <a href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_endangered_species_resolve_sors_5994_7593en_agilent_9a8507f587.pdf">Detection of Endangered Species Using the Agilent Resolve Raman Analyzer</a></strong></h4>
<ul>
<li>Application</li>
</ul>
<p><strong>Abstract:</strong> The Agilent Resolve handheld Raman system is a versatile analyzer that can be deployed on location to identify a broad range of materials. It uses traditional surface analysis mode and through-barrier mode through Agilent&#39;s proprietary spatially offset Raman spectroscopy (SORS) technology. SORS enables samples that are concealed behind barriers such as colored and opaque plastics, paper, and highly pigmented paints and varnishes to be identified. This application note details how the Resolve Raman system can be used to detect concealed endangered species products using SORS. Data are presented that show the effectiveness of Resolve operating in traditional surface mode to distinguish ivory from a plastic substitute. Further analysis of endangered animal products using surface mode enabled the division of animal products into two broad categories: mineral-based and protein-based. Principal components analysis (PCA) was used to further differentiate the protein-based samples, which included pangolin scale, rhino horn, dried seahorse, and totoaba fish bladder, based on their spectral differences.</p>
<p><strong>Conclusion:</strong>  The Agilent Resolve handheld Raman analyzer includes various spectral libraries that enable the identification of a broad range of chemicals and materials. This study has shown the application of the instrument and the SORS technique for the detection of endangered animal species. Using a combination of conventional surface and through-barrier modes of analysis, Raman spectroscopy and SORS technology can be used to:</p>
<ul>
<li>Identify ivory through layers of paint and varnish.</li>
<li>Differentiate plastic substitute materials from authentic ivory and bone.</li>
<li>Distinguish between mineral-based animal products, such as ivory and armadillo scale, from protein-based animal products, such as rhino horn and pangolin scales.</li>
</ul>
<p>The simple-to-use Resolve handheld Raman analyzer with SORS capability can provide complimentary data to help detect and identify endangered animal-derived samples.</p>
<h4><strong>5. Agilent Technologies: <a href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_raw_materials_synthetic_peptide_production_vaya_5994_7610en_agilent_b26123385c.pdf">Verification of Raw Materials for Synthetic Peptide Production with the Agilent Vaya Raman System</a></strong></h4>
<ul>
<li>Application</li>
</ul>
<p><strong>Abstract:</strong> Advancements in the manufacturing technology of peptide drug products have enabled large-scale synthetic peptide production, producing high-purity synthetic peptides in bulk. The widespread demand for glucagon-like peptide receptor agonists (GLP-1 RAs) has put pressure on synthetic peptide manufacturing capacity and revealed the need for efficient and scalable tools. The Agilent Vaya Raman raw material identity verification system enables uniquely efficient raw material verification due to its through-container identification capabilities. This application note showcases Vaya&#39;s successful through-container identification and differentiation of key building blocks for synthetic peptide manufacturing: fluorenylmethoxycarbonyl (Fmoc)-protected amino acids.</p>
<p><strong>Conclusion:</strong> The increasing demand for peptide biologics, such as GLP-1 receptor agonists, is expected to continue growing and outpacing current manufacturing capacity. To effectively meet demand, scalable solutions like the Agilent Vaya Raman raw material identity verification system introduce efficiencies to avoid bottlenecks that could be faced in raw material identification and regulatory-enforced verification. Additionally, the Vaya&#39;s ability to perform nondestructive, noninvasive identification ensures that raw materials are transferred expediently to production while preserving their integrity. </p>


News from LabRulezICPMS - Library Week 32, 2024

<p><strong>In the 2 weeks from August 19, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.</strong></p>
<blockquote>
<h4><a href="https://gcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4>
</blockquote>
<blockquote>
<p><strong>👉 Search and filter in the largest global database</strong>  with over <strong>3 500 GC, LC, MS and spectroscopy webinars</strong>.</p>
</blockquote>
<h5><strong>1. Agilent Technologies/Markes International: Environmental Air Monitoring: Methodologies, Regulations, and Market Trends</strong></h5>
<ul>
<li>Tu, 20.8.2024 10:30 CEST</li>
<li><a href="https://gcms.labrulez.com/webinar/4187">Registration</a></li>
</ul>
<p>An in-depth webinar on environmental air quality monitoring application solutions, organized by Agilent Technologies in collaboration with Markes International.</p>
<h5><strong>2. Wasson-ECE Instrumentation: Single Cylinder Sample Heater (New Product)</strong></h5>
<ul>
<li>Tu, 27.8.2024 21:30 CEST</li>
<li><a href="https://gcms.labrulez.com/webinar/4216">Registration</a></li>
</ul>
<p>Please join us for an introduction to Wasson&#39;s new Single Cylinder Heater/Auto Sampler.</p>
<h5><strong>3. Thermo Fisher Scientific: Improved EA-IRMS NCS workflow for archaeology and ecology applications</strong></h5>
<ul>
<li>We, 28.8.2024 16:00 CEST</li>
<li><a href="https://gcms.labrulez.com/webinar/4210">Registration</a></li>
</ul>
<p>This presentation will describe how we have optimized our Thermo Scientific EA IsoLink System with the new High Performance Kit for sulfur analysis to allow for high precision and accuracy NCS analysis.</p>
<h5><strong>4. LECO: Non-targeted screening in forensics, a discussion of method development and screening of forensic samples using GCXGC-TOFMS</strong></h5>
<ul>
<li>Th, 29.8.2024 14:00 CEST</li>
<li><a href="https://gcms.labrulez.com/webinar/4212">Registration</a></li>
</ul>
<p>Non-targeted screening in forensics, a discussion of method development and screening of forensic samples using GCXGC-TOFMS.</p>


Webinars LabRulezGCMS Week 34-35/2024

<p><strong>In the week of August 19, the following webinars await you in the field of liquid phase and especially HPLC and LC/MS.</strong></p>
<blockquote>
<h4><a href="https://lcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4>
</blockquote>
<blockquote>
<p><strong>👉 Search and filter in the largest global database</strong>  with over <strong>3 500 GC, LC, MS and spectroscopy webinars</strong>.</p>
</blockquote>
<h5><strong>1. Agilent Technologies: Elevate Your Protein Characterization: Discover Agilent ExD</strong></h5>
<ul>
<li>Tu, 20.8.2024 06:30 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/4198">Registration</a></li>
</ul>
<p>Learn how you can meet these challenges with the latest enhancements for peptide &amp; protein characterization with the Agilent 6545XT AdvanceBio LC/Q-TOF.</p>
<h5><strong>2. SCIEX: SCIEX OS software summer school - Data processing: quantitation</strong></h5>
<ul>
<li>Tu, 20.8.2024 11:00 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/4157">Registration</a></li>
</ul>
<p>Join us for our summer school series dedicated to enhancing your proficiency with SCIEX OS software.</p>
<h5><strong>3. Agilent Technologies: Reaching Ultra-Trace PFAS Detection Limits by Overcoming Solvent Effects at High Injection Volumes</strong></h5>
<ul>
<li>We, 21.8.2024 17:00 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/4165">Registration</a></li>
</ul>
<p>High concentration factor in sample preparation with the use of Feed Injection for improved chromatographic performance at high injection volumes and with LC/MS allows lowest possible PFAS detection limits.</p>
<h5><strong>4. Thermo Fisher Scientific: Single-cell spatial metabolomics and lipidomics using AP-SMALDI and Orbitrap technology</strong></h5>
<ul>
<li>Th, 22.8.2024 11:00 CEST</li>
<li><a href="https://lcms.labrulez.com/webinar/4188">Registration</a></li>
</ul>
<p>Technical aspects of mass spectrometry imaging, including the use of a specialized objective lens and the importance of high lateral resolution and mass resolving power.</p>


Webinars LabRulezLCMS Week 34/2024

<p><strong>In the week from August 19, the following webinars await you in the field of atomic and molecular spectroscopy and spectrometry</strong></p>
<blockquote>
<h4><a href="https://icpms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4>
</blockquote>
<blockquote>
<p><strong>👉 Search and filter in the largest global database</strong>  with over <strong>3 500 GC, LC, MS and spectroscopy webinars</strong>.</p>
</blockquote>
<h5><strong>1. SelectScience/CYTEK: Improving Results Through Better Understanding: A Primer On High-Dimensional Flow Cytometry Technologies And Reagents</strong></h5>
<ul>
<li>Tu, 20.8.2024 17:00 CEST</li>
<li><a href="https://icpms.labrulez.com/webinar/4186">Registration</a></li>
</ul>
<p>A broad overview of available high-dimensional flow cytometry technologies and reagents, how they work, and an experience-informed breakdown of the strengths and limitations of each technique. </p>
<h5><strong>2. Agilent Technologies: Analysis of Electrolyte and Li salts commonly used in Li Battery manufacturing</strong></h5>
<ul>
<li>Tu, 20.8.2024 21:30 CEST</li>
<li><a href="https://icpms.labrulez.com/webinar/3910">Registration</a></li>
</ul>
<p>Analysis of Electrolyte and Li salts commonly used in Li Battery manufacturing.</p>
<h5><strong>3. Agilent Technologies: The benefits of a fully Integrated Advanced Dilution System (ADS) for ICP-OES</strong></h5>
<ul>
<li>Th, 22.8.2024 20:00 CEST</li>
<li><a href="https://icpms.labrulez.com/webinar/3911">Registration</a></li>
</ul>
<p>Boost productivity and eliminate tedious standard and sample preparation using Agilent’s Advanced Dilution System (ADS) with the ICP-OES.</p>


Webinars LabRulezICPMS Week 34/2024

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LECO Training Course CS-744/844 Series & ON/ONH-736/836 Series

SCIEX at SOFT/TIAFT

Waters at SOFT/TIAFT 2026

Automatic ICP-OES Analysis of Lubricating Oils Using SPECTRO GENESIS DSOI and ACAROS Automation

Detection and Identification of Microplastics in Water and Other Matrices Using the Agilent Laser Infrared Spectroscopy Microscope

Unlocking New Analytical Possibilities with Waters APGC Solutions